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Preparation method of polyacid-like late transition metal-organic network catalyst material

A late-transition metal, organic network technology is applied in the field of preparation of late-transition metal-organic network catalyst materials, and can solve the problems of difficult to control synthesis, shedding, etc.

Inactive Publication Date: 2013-06-26
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalysts obtained by the above methods may encounter the following unfavorable factors: homogeneous form, difficult to control the synthesis, active sites fall off from the support, preventing substrates from accessing catalytic active sites, etc.

Method used

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  • Preparation method of polyacid-like late transition metal-organic network catalyst material
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  • Preparation method of polyacid-like late transition metal-organic network catalyst material

Examples

Experimental program
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Effect test

Embodiment 1

[0019] A late-transition metal-organic network catalyst material of a class of polyacids, the chemical composition of which is: [Zn 16 (HPO 3 ) 4 ] L 3 .

[0020] Preparation method: Grind molybdate and molybdenum powder evenly at a molar ratio of 5:1, add zinc salt, phosphorous acid, organic bridging ligand and water (10 ml), and stir for 15 minutes. Then adjust the pH of the mixture to 5 with dilute hydrochloric acid, put it into a high-pressure reactor, raise the temperature to 180°C at a rate of 1-5°C / min, keep it warm for 48 hours, and then cool it down to room temperature at a rate of 1-5°C / min , and the catalyst was obtained by filtration.

Embodiment 2

[0022] A late-transition metal-organic network catalyst material of a class of polyacids, the chemical composition of which is: [Cd 16 (HPO 3 ) 4 ] L 3 .

[0023] Preparation method: Grind molybdate and molybdenum powder evenly at a molar ratio of 5:1, add cadmium salt, phosphorous acid, organic bridging ligand and water (10 ml), and stir for 30 minutes. Then adjust the pH value of the mixture to 4 with dilute hydrochloric acid, put it into a high-pressure reactor, raise the temperature to 180°C at a rate of 1-5°C / min, keep it warm for 72 hours, and then lower it to room temperature at a rate of 1-5°C / min , and the catalyst was obtained by filtration.

Embodiment 3

[0025] A late-transition metal-organic network catalyst material of a class of polyacids, the chemical composition of which is: [Cu 16 (HPO 3 ) 4 ] L 3 .

[0026] Preparation method: Grind molybdate and molybdenum powder evenly at a molar ratio of 5:1, add copper salt, phosphorous acid, organic bridging ligand and water (10 ml), and stir for 60 minutes. Then adjust the pH of the mixture to 6 with dilute hydrochloric acid, put it into a high-pressure reactor, raise the temperature to 180°C at a rate of 1-5°C / min, keep it warm for 60 hours, and then lower it to room temperature at a rate of 1-5°C / min. The catalyst was obtained by filtration.

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Abstract

The invention belongs to a chemical synthesis method and in particular relates to a preparation method of a polyacid-like late transition metal-organic network catalyst material. The polyacid-like late transition metal-organic network catalyst material has a (3,4,24)-connecting topological polyacid-like salt-organic compound structure, is a crystalline catalyst which is obtained by converting a late transition metal salt and an organic bridging ligand into a metal organic network under appropriate pH and temperature, and has a chemical component of [M16(HPO3)4]L3, wherein L is the organic bridging ligand, and M contains Zn, Cd, Cu, Co, Ni and the like. The polyacid-like late transition metal-organic network catalyst is a late transition metal oxygen cluster and breaks through the traditional polyacid limit; and as late transition metal ions are introduced into the catalyst, the stability, selectivity and catalytic activity of the catalyst can be effectively improved.

Description

technical field [0001] The invention belongs to a chemical synthesis method, in particular to a preparation method of a polyacid-like post-transition metal-organic network catalyst material. Background technique [0002] Polyacids, that is, anionic metal oxide clusters (POM), are a class composed of d 0 or d 1 Electron-configured early-transition metals and oxygen-formed polymetallic oxygen clusters. The chemistry of polyacids has attracted much attention in the past two decades, not only because of their fascinating structural and electronic properties, but also because of their wide-ranging applications ranging from catalysis to medicine. completely by d 10 The POM clusters constructed by late-transition metals in electronic configuration will be unstable due to high negative charge and difficult to be separated, although a series of late-transition metal ions (such as Fe 3+ , Co 2+ , Cu 2+ , Mn 2+ and Zn 2+ ) substituted polyacid clusters are often reported. Comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22
Inventor 秦俊生杜东英兰亚乾苏忠民
Owner NORTHEAST NORMAL UNIVERSITY
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